HRID2077802
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
A mixture of 2-(4-{[5-chloro-2-{[4-(4-pyridinyl)butanoyl]amino}-4-(trifluoromethyl)phenyl]amino}phenyl)ethyl acetate (step 3, 220 mg, 0.42 mmol) and 2N NaOH (15 ml) in ethanol (20 ml) was stirred at 40° C. for 7 h. The solvent was removed and the residue was added water (50 ml). The mixture was extracted with ethyl acetate (100 ml). The organic layer was washed with brine (50 ml), then dried (Na2SO4). After removal of solvent, the crude product was purified by flash column chromatography eluting with dichloromethane:methanol (20:1) to afford 105 mg (54%) of the title compound as pale brown oil.
WORKUP
后处理
- customThe solvent was removed
- additionthe residue was added water (50 ml)
- extractionThe mixture was extracted with ethyl acetate (100 ml)
- washThe organic layer was washed with brine (50 ml)
- dry with materialdried (Na2SO4)
- customAfter removal of solvent
- customthe crude product was purified by flash column chromatography
- washeluting with dichloromethane:methanol (20:1)